U.S. patent application number 12/797828 was filed with the patent office on 2010-09-30 for combinatorial deposition method and apparatus thereof.
Invention is credited to Masahiro GOTO, Akira Kasahara, Masahiro Tosa.
Application Number | 20100242837 12/797828 |
Document ID | / |
Family ID | 35320250 |
Filed Date | 2010-09-30 |
United States Patent
Application |
20100242837 |
Kind Code |
A1 |
GOTO; Masahiro ; et
al. |
September 30, 2010 |
COMBINATORIAL DEPOSITION METHOD AND APPARATUS THEREOF
Abstract
A combinatorial deposition method is characterized in that, in a
method of performing thin-film coating onto a substrate disposed in
a vacuum, two or more substrates are moved between a deposition
position and a cooling position, sequentially only substrates to be
coated is moved to the deposition position while substrates at the
cooling position are cooled by a cooling mechanism, and substrates
are respectively deposited under different deposition conditions in
only one vacuum evacuation process. Various deposition conditions
with regard to sputtering and the like are accurately controlled,
so that coating films can be efficiently produced under different
deposition conditions.
Inventors: |
GOTO; Masahiro;
(Tsukuba-shi, JP) ; Kasahara; Akira; (Tsukuba-shi,
JP) ; Tosa; Masahiro; (Tsukuba-shi, JP) |
Correspondence
Address: |
WENDEROTH, LIND & PONACK, L.L.P.
1030 15th Street, N.W.,, Suite 400 East
Washington
DC
20005-1503
US
|
Family ID: |
35320250 |
Appl. No.: |
12/797828 |
Filed: |
June 10, 2010 |
Related U.S. Patent Documents
|
|
|
|
|
|
Application
Number |
Filing Date |
Patent Number |
|
|
12554299 |
Sep 4, 2009 |
|
|
|
12797828 |
|
|
|
|
10553848 |
Dec 14, 2005 |
|
|
|
PCT/JP2004/015857 |
Oct 20, 2004 |
|
|
|
12554299 |
|
|
|
|
Current U.S.
Class: |
118/50 ;
204/298.07; 204/298.15 |
Current CPC
Class: |
C23C 14/35 20130101;
C23C 14/5806 20130101; C23C 14/541 20130101; C23C 14/56 20130101;
C23C 14/3492 20130101 |
Class at
Publication: |
118/50 ;
204/298.07; 204/298.15 |
International
Class: |
C23C 14/34 20060101
C23C014/34; C23C 14/00 20060101 C23C014/00 |
Foreign Application Data
Date |
Code |
Application Number |
May 10, 2004 |
JP |
2004-139866 |
Claims
1-5. (canceled)
6. A combinatorial deposition apparatus characterized in that the
apparatus performs thin-film coating onto a substrate disposed in a
vacuum, wherein a sample holder can hold two or more substrates,
and each substrate can be moved to a deposition position or a
cooling position, and sequentially only substrates to be coated are
moved to the deposition position and subjected to deposition while
substrates at the cooling position are cooled by a cooling
mechanism, in one vacuum evacuation process.
7. The combinatorial deposition apparatus according to claim 6,
characterized in that deposition is performed for the two or more
substrates with different deposition conditions for each
substrate.
8. The combinatorial deposition apparatus according to claim 6
characterized in that the two or more substrates can be moved to
the deposition position or the cooling position by a rotation
mechanism.
9. The combinatorial deposition apparatus according to claim 6
characterized in that even if a substrate at the deposition
position is heated to 1000.degree. C. or more, rise in temperature
of substrates at the cooling position can be restrained within 100
K.
10. The combinatorial deposition apparatus according to claim 6
characterized in that a water- or liquid nitrogen-cooling mechanism
is used.
11. The combinatorial deposition apparatus according to claim 6,
characterized in that the apparatus is for deposition by
sputtering, and deposition can be performed for two or more
substrates with any one or more of the following deposition
conditions: sputter gas pressure, sputter gas, partial pressure,
sputter power value, substrate temperature, distance between the
substrate and target, and sample bias, which are varied for each
substrate, in one vacuum evacuation process.
12. The combinatorial deposition apparatus according to claim 11,
characterized in that a valve for controlling the sputter gas
pressure has a feedback function of changing conductance so that
the pressure is equal to a prescribed value.
13. The combinatorial deposition apparatus according to claim 11,
characterized in that the distance between the substrate and the
target can be controlled by a straight-line introducing
mechanism.
14. The combinatorial deposition apparatus according to claim 6,
characterized in that a turbo molecular pump is provided as a
vacuum evacuation mechanism.
15. The combinatorial deposition apparatus according to claim 6,
characterized in that a substrate suited for the Suzuki friction
test can be mounted.
16. The combinatorial deposition apparatus according to claim 6,
characterized in that a position of the sample holder or a sputter
source is variable, wherein deposition can be performed for a
substrate cooled by the cooling mechanism.
17-19. (canceled)
Description
TECHNICAL FIELD
[0001] The present invention relates to a combinatorial deposition
method and an apparatus thereof. More particularly, the invention
relates to a combinatorial deposition method and an apparatus
thereof in which various sputter deposition conditions can be
accurately controlled, and coating films can be efficiently
prepared under different deposition conditions.
BACKGROUND ART
[0002] Thin film coating onto a substrate is one effective material
development method for enhancing the excellent function of a
substrate material, adding a new function, or further increasing
the life of the substrate material, and it is now drawing attention
for its application in industrial, biological, aerospace, and other
various fields. For investigation of various thin layer
compositions of such thin film coatings, a deposition apparatus
using a combinatorial method, and a masking mechanism that can
prepare a thin film in correspondence with a 3-dimensional diagram
have been proposed (e.g. patent document 1), and thus thin film
composition that can generate new properties can be efficiently
found.
[0003] On the other hand, for the investigation of thin film
conditions, experiments and evaluations of many kinds of deposition
conditions are needed in which a large number of deposition
condition parameters are changed little by little. Thus, the best
conditions have not been able to be determined without tremendous
labor, time and other difficulties. For example, in thin film
coating prepared by sputtering, properties of obtained coating
films are largely influenced by many deposition condition
parameters such as sputter gas pressure, gas type, partial
pressure, sputter power value, substrate temperature, distance
between the substrate and a target, and sample bias, in addition to
the composition and combination of sputter materials. Therefore,
although experiments are need in which each of the deposition
condition parameters is changed for determining the best
conditions, actually in most cases evaluation has been conducted on
experiments where only one or two kinds of deposition condition
parameters are changed. Accordingly, it is highly unlikely that the
deposition conditions have been optimized with regard to all the
various properties of the obtained coating films.
[0004] Patent document 1: JP-A-2004-035983.
[0005] However, if the thin film coating were performed under many
deposition conditions whose parameters are accurately controlled,
and characteristics of the coating films are evaluated, the best
deposition conditions that optimize each of the properties of the
coating films could be determined. Therefore, a deposition method
and an apparatus in which the parameters can be controlled
accurately and efficiently are desired.
[0006] Thus, the subject of the invention of the application, which
was made in the light of the above circumstances, is to provide a
method and an apparatus thereof, in which the problems in the
conventional art are solved, many deposition condition parameters
of sputter coating and the like can be accurately controlled, and
many kinds of coating films under different deposition conditions
are produced efficiently with the parameters being changed little
by little. Such combinatorial deposition is realized, thereby the
optimum conditions of each of the properties (frictional property,
electrical conductivity, optical property, thermal property and the
like) of the coating films can be easily determined, which is
extremely useful for developing a new material.
DISCLOSURE OF THE INVENTION
[0007] To solve the above problems, first, the present invention
provides a combinatorial deposition method characterized in that,
in a method for performing the thin-film coating onto a substrate
disposed in vacuum, two or more substrates can be moved to a
deposition position or a cooling position, and in one vacuum
evacuation process, while substrates are held at the cooling
position where the substrates are cooled by a cooling mechanism,
only objective substrates to be coated are sequentially moved to
the deposition position and subjected to deposition.
[0008] Second, the present invention provides a combinatorial
deposition method characterized in that the deposition is performed
to two or more substrates with the deposition conditions different
for each substrate; third, it provides a combinatorial deposition
method characterized in that the two or more substrates can be
moved to the deposition position or the cooling position by a
rotation mechanism; fourth, it provides a combinatorial deposition
method characterized in that a water- or liquid nitrogen-cooling
mechanism is adopted; fifth, it provides a combinatorial deposition
method characterized in that the deposition is performed by
sputtering with any one or more of the following deposition
conditions: sputter gas pressure, sputter gas, partial pressure,
sputter power value, substrate temperature, distance between a
substrate and a target, and sample bias, and the conditions are
different for each substrate in one vacuum evacuation process.
[0009] Furthermore, sixth, the invention of the present application
provides a combinatorial deposition apparatus characterized in that
the apparatus performs thin-film coating onto the substrate
disposed in a vacuum, wherein a sample holder can hold two or more
substrates, and each substrate can be moved to a deposition
position or a cooling position, and in one vacuum evacuation
process, while substrates at the cooling position are cooled by the
cooling mechanism, only objective substrates to be coated are
sequentially moved to the deposition position and subjected to
deposition.
[0010] Moreover, seventh, the invention of the application provides
a combinatorial deposition apparatus characterized in that the
deposition is performed on the two or more substrates with the
deposition conditions different for each substrate; eighth, it
provides a combinatorial deposition apparatus characterized in that
the two or more substrates can be moved to the deposition position
or the cooling position by a rotation mechanism; ninth, it provides
a combinatorial deposition apparatus characterized in that even if
the substrate at the deposition position is heated to 1000.degree.
C. or more, the rise in temperature in the substrates at the
cooling position can be restrained within 100 K; tenth, it provides
combinatorial deposition apparatus characterized in that a water-
or liquid nitrogen-cooling mechanism is adopted as a cooling
mechanism; eleventh, it provides combinatorial deposition apparatus
characterized in that the apparatus is for deposition by
sputtering, wherein in one vacuum evacuation process, deposition
can be performed for two or more substrates by varying any one or
more of the following deposition conditions: sputter gas pressure,
sputter gas type, partial pressure, sputter power value, substrate
temperature, distance between a substrate and a target, and sample
bias; twelfth, it provides combinatorial deposition apparatus
characterized in that a valve for controlling sputter gas pressure
is provided and a feedback mechanism changing conductance so as to
control the sputter gas pressure at a prescribed value is provided;
thirteenth, it provides combinatorial deposition apparatus
characterized in that the distance between the substrate and the
target can be controlled by a straight-line introducing mechanism;
fourteenth, it provides a combinatorial deposition apparatus
characterized in that a turbo molecular pump is provided as a
vacuum evacuation mechanism; fifteenth, it provides a combinatorial
deposition apparatus characterized in that a substrate for
Suzuki-type friction test can be mounted; and sixteenth, it
provides a combinatorial deposition apparatus characterized in that
a position of the sample holder or a sputter source is variable,
and deposition can be performed for a substrate cooled by the
cooling mechanism.
[0011] In addition, seventeenth, the invention of the application
provides a sample holder characterized in that the sample holder
has a rotation mechanism that can hold two or more samples, wherein
while a sample not to be subjected to deposition is cooled at the
cooling position by the cooling mechanism, only a sample to be
subjected to deposition is subjected to temperature control at the
deposition position; eighteenth, it provides a sample holder
characterized in that even if the substrate at the deposition
position is heated to 1000.degree. C. or more, the rise in
temperature of the substrates at the cooling position can be
restrained within 100.degree. K.; and nineteenth, it provides a
sample holder characterized in that a water- or liquid
nitrogen-cooling mechanism is adopted as the cooling mechanism.
BRIEF DESCRIPTION OF THE DRAWINGS
[0012] FIG. 1 is a view schematically illustrating a general
configuration of a combinatorial coating apparatus of the invention
of the application;
[0013] FIG. 2 is a graph illustrating change in friction
coefficient of a thin film deposited with different substrate
temperature using a combinatorial coating apparatus of the
invention of the application; and
[0014] FIG. 3 is a graph illustrating change in friction
coefficient of a thin film deposited with different oxygen partial
pressure using a combinatorial coating apparatus of the invention
of the application.
REFERENCES IN THE FIGURES INDICATE AS FOLLOWS
[0015] 1 chamber, [0016] 2 sample holder, [0017] 3 sputter source,
[0018] 4 evacuation system, [0019] 5 inert-gas supply port, [0020]
6 reactive-gas supply port, [0021] 7 heater, [0022] 8 cooling
mechanism, [0023] 9 valve, [0024] 11 view port, and [0025] 21
substrate.
DETAILED DESCRIPTION OF THE INVENTION
[0026] The invention of the present application has the
aforementioned features, and hereinafter, several embodiments are
described. The most distinctive feature is that, in the invention
of the application, deposition can be performed under various
deposition conditions in one vacuum evacuation process.
Accordingly, deposition according to a combinatorial manner in
which many deposition conditions are changed little by little can
be realized accurately and simply.
[0027] A combinatorial deposition method of the invention of the
present application is characterized in that in a method of thin
film coating a substrate disposed in a vacuum, it is possible for
two or more substrates to be moved to the deposition position or
the cooling position, and in one vacuum evacuation process, only
objective substrates to be coated are sequentially moved to the
deposition position and subjected to deposition, while the
substrates at the cooling position are cooled by the cooling
mechanism.
[0028] As the method of thin film coating onto the substrate
disposed in a vacuum, to which the combinatorial deposition method
of the present invention is applied, various known deposition
methods including physical vapor deposition (PVD) such as sputter
or vacuum evaporation, and chemical vapor deposition (CVD) such as
thermal decomposition reaction, reactive evaporation and chemical
transport, can be used. More specifically, for example, magnetron
sputter, molecular beam epitaxy, or pulse laser evaporation can be
considered.
[0029] In the combinatorial deposition method of the application,
to perform the deposition for two or more substrates, each
substrate can be moved to a deposition position or a cooling
position. Then, in one vacuum evacuation process, only objective
substrates to be coated are sequentially moved to the deposition
position and subjected to the deposition while the substrates at
the cooling position are cooled by the cooling mechanism. The
number of substrates is not particularly limited, and can be
appropriately determined in consideration of substrate size, size
of apparatus for deposition, the number of deposition conditions
and the like. As moving means of the two or more substrates, which
is not particularly limited, various mechanisms and structures can
be considered. For example, a moving means using a rotation
mechanism such as turntable, a belt conveyer, and further a moving
means having an up-and-down function can be exemplified. In
addition, a cooling mechanism is not particularly limited, and for
example, cooling using a refrigerant such as liquid nitrogen,
liquid helium, or water can be exemplified. In particular, in the
invention of the application, a water cooling mechanism with water
circulation or liquid-nitrogen cooling mechanism is simple and
preferable.
[0030] For the substrate at the deposition position, substrate
temperature can be controlled according to deposition conditions.
Specifically, for example, the substrate can be subjected to
deposition while being heated, or the substrate can be subjected to
deposition without heating, or the substrate can be also subjected
to deposition while being cooled.
[0031] In this way, deposition is sequentially performed for only
objective substrates to be coated, while other substrates are
cooled, so that deposition can be performed for two or more
substrates in one vacuum evacuation process. In deposition,
deposition conditions can be changed for each substrate. Thus, in
one vacuum evacuation process, deposition according to a
combinatorial manner in which many deposition conditions are
changed little by little can be realized.
[0032] More specifically, for example, regarding deposition by
sputtering, in the combinatorial deposition method of the invention
of the application, deposition can be performed for many substrates
with varying any one or more of the following deposition conditions
in one vacuum evacuation process: sputter gas pressure, sputter gas
type, partial pressure, sputter power value, substrate temperature,
distance between a substrate and a target.
[0033] The combinatorial deposition method as above can be simply
realized by a combinatorial deposition apparatus provided by the
invention of the application. Thus, the combinatorial deposition
apparatus of the invention of the application is characterized in
that the apparatus is for performing thin film coating for the
substrates disposed in vacuum, wherein a sample holder can hold two
or more substrates and move each substrate to a deposition position
or a cooling position, and only objective substrates to be coated
are sequentially moved to the deposition position and subjected to
the deposition while the substrates at the cooling position are
cooled by the cooling mechanism, in one vacuum evacuation
process.
[0034] The combinatorial deposition apparatus of the invention of
the application have various configurations according to various
thin-film coating methods, but the sample holder is distinctive. In
the sample holder, two or more substrates can be held and each
substrate can be moved to a deposition position or a cooling
position. The number of substrates that can be held is not
particularly limited, and can be appropriately determined in
consideration of the size of a substrate, size of an apparatus for
deposition, the number of deposition conditions and the like. The
sample holder is exchangeable according to conditions such as a
substrate. A moving means of two or more substrates is not
particularly limited, and various mechanisms and structures can be
considered. For example, a moving means using a rotation mechanism
such as a turntable, a belt conveyer, or a moving means having an
up-and-down function can be exemplified. In the invention of the
application, it is simple and preferable that two or more
substrates can be moved to a deposition position or a cooling
position by a rotation mechanism. Moreover, a cooling mechanism is
not particularly limited, and for example, cooling using a
refrigerant such as liquid nitrogen, liquid helium, or water can be
exemplified. In the invention of the application, a water cooling
mechanism with water circulation or a liquid nitrogen cooling
mechanism is illustrated as a simple and preferable example.
[0035] Thus, for example, a sample holder provided by the invention
of the application is characterized in that the sample holder has a
rotation mechanism that can hold two or more samples, wherein it is
possible for samples not to be coated to be cooled by a cooling
mechanism at a cooling position, and for only samples to be coated
to be subjected to temperature control at a deposition position.
More specifically, for example, as illustrated in FIG. 1, a sample
holder (2) has a turntable, and substrates (21) are disposed on the
turntable in an approximately circular pattern. Near a deposition
position, a heater (7) for heating is arranged and near cooling
positions, a cooling mechanism (8) with a cooling pipe is arranged,
so that temperature of the substrate (21) at the deposition
position can be controlled to a desired deposition temperature and
then subjected to the deposition while substrates (21) at the
cooling position are cooled. According to the configuration, for
example, even if the substrate (21) at the deposition position is
heated to 1000.degree. C. or more, the rise in temperature of the
substrates (21) at the cooling position can be restrained within
100 K. Moreover, since the substrate (21) can be moved between the
deposition position and the cooling position by rotating the
turntable, only the substrate (21) that is moved to the deposition
position is sequentially subject to deposition. Thus, deposition
can be performed by varying deposition conditions for each
substrate (21). Therefore, the sample holder (2) of the invention
of the application makes it possible to perform deposition
according to a combinatorial manner in various thin-film coating
method.
[0036] For example, a combinatorial deposition apparatus provided
by the invention of the application may be for deposition by
sputtering, wherein deposition can be performed for two or more
substrates by varying any one or more of the following deposition
conditions: sputter gas pressure, sputter gas, partial pressure,
sputter power value, substrate temperature, distance between a
substrate and a target, and sample bias, in one vacuum evacuation
process. The sputtering deposition apparatus may be, for example,
illustrated in FIG. 1, in which a sample holder (2) and a sputter
source (3) are installed in a chamber (1), and a vacuum evacuation
mechanism (4) and supply ports (5), (6) for inert gas and reactive
gas are provided. In such a combinatorial deposition apparatus, a
valve (9) for controlling sputter gas pressure may have a feedback
function for changing conductance so that the pressure becomes a
prescribed value. Sputter gas pressure can be set accurately and
reproducibly. The distance between the substrate (21) and a target
can be controlled by the straight-line introducing mechanism for
the sputter source (3). Furthermore, a turbo molecular pump and the
like are provided as the vacuum evacuation mechanism (4), so that,
for example, in a vacuum system of the apparatus, ultra high vacuum
of about 10.sup.-5 Pa can be realized in a shorter time. The sample
holder (2) is configured so that a substrate (21) suited for the
Suzuki friction test can be mounted, and thus various property
evaluation of coating thin-films produced can be performed more
simply.
[0037] The combinatorial deposition apparatus of the invention of
the application is further characterized in that a position of the
sample holder (2) or the sputter source (3) is variable and
deposition can be performed for a substrate (21) cooled by the
cooling mechanism (8). Thus, for example, by arranging a deposition
position near the cooling mechanism (8) and by changing a position
of the sample holder (2) or the sputter source (3), deposition can
be performed for a substrate (21) while being cooled.
[0038] According to the invention of the present application, by
changing various deposition conditions are changed little by
little, many coating thin-films different in natures such as
crystallinity and crystal orientation can be manufactured
efficiently. And by evaluating various properties such as
frictional properties, electrical conductivity, optical properties,
and thermal properties of the various obtained coatings, many
deposition condition parameters can be optimized more simply and
surely and possibility of development of a new functional coating
film is remarkably expanded.
[0039] Hereinafter, an embodiment of the invention of the
application is further described in detail. It goes without saying
that the invention is not limited to the following example and
various modifications are possible.
EXAMPLE
[0040] FIG. 1 is a view schematically illustrating a general
configuration of an example of a combinatorial coating apparatus of
the invention of the application. The combinatorial coating
apparatus is a deposition apparatus using magnetron sputter and is
composed of a main chamber (1), a multi-sample holder (2) and a
sputter source (3) built in the main chamber (1), a vacuum
evacuation system (4) connected to the main chamber (1), an
inert-gas supply port (5), a reactive-gas supply port (6) and the
like. A view port (11) of ICF305 size is provided at a front of the
main chamber (1), and thus the multi-sample holder (2) can be
efficiently taken in and out. Regarding the sputter gun (3), a
position can be changed using a straight-line introducing mechanism
(not shown), so that the distance between the substrate (21) to be
deposited and the target can be controlled. The vacuum evacuation
system (4) has a turbo molecular pump having throughput of 600 l/s,
which can perform vacuum evacuation of 10.sup.-5 Pa in a short
time. Regarding a valve (9) for communicating between the main
chamber (1) and the vacuum evacuation system (4), opening and
closing can be controlled by feedback that conductance is varied so
that a prescribed pressure is attained, and thereby accurate
setting of the sputter gas pressure can be achieved repeatedly.
[0041] A plural number of substrates (21), 14 in the case of FIG.
1, can be mounted on the multi-sample holder (2) and can be
sequentially moved by rotation using the rotation mechanism. A
substrate (21) to be deposited is moved to a deposition position
near a heater (7) and the other 13 substrates (21) are disposed at
a cooling position near a water cooling mechanism (8). Even if the
substrate (21) to be deposited is heated to approximately
1000.degree. C. by the heater (7), the other 13 samples are cooled
by the cooling mechanism (8), so that the rise in temperature of
these samples can be restrained within 100 K and only the objective
substrate (21) can be deposited. According to such a configuration,
deposition conditions can be accurately varied for each substrate
(21) and, for example, 14 kinds of deposition conditions are
realized in one vacuum evacuation process. Since the multi-sample
holder (2) can be mounted with a substrate suited for the Suzuki
friction test, property tests of coating films deposited can be
efficiently conducted.
[0042] The change in friction coefficients of the films produced
under various deposition conditions using the combinatorial coating
apparatus described above was examined. FIG. 2 illustrates change
in friction coefficient in the case where deposition was performed
under 8 different substrate temperatures. FIG. 3 illustrates change
in friction coefficient in the case where deposition was performed
under 8 different oxygen partial pressures. Furthermore, change in
friction coefficient could be examined in the case that deposition
was performed under different substrate temperatures and different
partial pressures. In this way, respective thin films deposited
under different deposition conditions can be obtained in one vacuum
evacuation process, and evaluation of various properties of the
obtained coating films and optimization of the deposition
conditions of the films can be easily performed.
INDUSTRIAL APPLICABILITY
[0043] According to the invention of the application, a
combinatorial deposition method and an apparatus thereof are
provided, in which various conditions for deposition by sputtering
and the like can be accurately controlled, and coating films can be
efficiently produced under different deposition conditions.
* * * * *